홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Ninhydrin → Tacrolimus

HRID 1991024
노트
인쇄 미리보기

반응식

HRID 1991024 반응식
[CH2:1]([CH:4]1[CH:30]=[C:29]([CH3:31])[CH2:28][CH:27]([CH3:32])[CH2:26][CH:25]([O:33][CH3:34])[CH:24]2[O:35][C:20]([OH:39])([CH:21]([CH3:38])[CH2:22][CH:23]2[O:36][CH3:37])[C:19](=[O:40])[C:18](=[O:41])[N:17]2[CH:12]([CH2:13][CH2:14][CH2:15][CH2:16]2)[C:11](=[O:42])[O:10][CH:9]([C:43]([CH3:65])=[CH:44][CH:45]2[CH2:50][CH2:49][CH:48]([O:51]C(=O)CCCCCCC(O)=O)[CH:47]([O:63][CH3:64])[CH2:46]2)[CH:8]([CH3:66])[CH:7]([OH:67])[CH2:6][C:5]1=[O:68])[CH:2]=[CH2:3].CCN=C=NCCCN(C)C.ON1C2C=CC=CC=2N=N1.C1C=C2C(C(O)(O)C(=O)C2=CC=1)=O.C(OC(=O)C)(=O)C.CN(C)C=O>C(Cl)Cl.CN1CCCC1=O.C1C=CC=CC=1>[CH3:32][C@H:27]1[CH2:28][C:29]([CH3:31])=[CH:30][C@@H:4]([CH2:1][CH:2]=[CH2:3])[C:5](=[O:68])[CH2:6][C@H:7]([OH:67])[C@@H:8]([CH3:66])[C@@H:9](/[C:43](/[CH3:65])=[CH:44]/[C@H:45]2[CH2:46][C@@H:47]([O:63][CH3:64])[C@H:48]([OH:51])[CH2:49][CH2:50]2)[O:10][C:11](=[O:42])[C@H:12]2[N:17]([CH2:16][CH2:15][CH2:14][CH2:13]2)[C:18](=[O:41])[C:19](=[O:40])[C@:20]2([OH:39])[O:35][C@@H:24]([C@@H:23]([O:36][CH3:37])[CH2:22][C@H:21]2[CH3:38])[C@@H:25]([O:33][CH3:34])[CH2:26]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 10236NinhydrinHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 72524391HCID 72524391, 화합물HCID 86761394acetic anhydride DMF

생성물 1

HCID 445643Tacrolimus

시약·촉매·용매 2

HCID 241Benzene용매HCID 19383075dichloromethane N-methyl-2-pyrrolidone용매

실험 절차

The syrup obtained in Example 1 was centrifuged with benzene and concentrated under reduced pressure, and dissolved in a mixed solvent of methylene chloride/N-methyl-2-pyrrolidone (4/1) (0.3 ml), and WSC (1.44 mg, 7.5 μmol) and 1-hydroxybenzotriazole (1.01 mg, 7.5 μmol) were added. This solution was added to 10 μl of TOYO-Pearl resin (TSKgel AF-amino; 0.01 mmol amine is present in 100 μl) and shaken at room temperature overnight. After completion of the reaction, the resin was thoroughly washed with a mixed solvent of methylene chloride/N-methyl-2-pyrrolidone (4/1), and DMF, and the percent condensation yield was determined by the ninhydrin test (about 29%). A mixed solution of acetic anhydride/DMF (1/4) (0.3 ml) was added to the resin obtained, and this was followed by shaking at room temperature for 30 minutes. After completion of the reaction, the resin was thoroughly washed with methylene chloride, dimethylformamide (DMF) and 20% aqueous ethanol, and this resin was used as the affinity resin in the subsequent experiments.

후처리

  1. concentrationconcentrated under reduced pressure
  2. additionwere added
  3. customAfter completion of the reaction
  4. washthe resin was thoroughly washed with a mixed solvent of methylene chloride/N-methyl-2-pyrrolidone (4/1), and DMF
  5. customthe percent condensation
  6. customyield
  7. customobtained
  8. stirringby shaking at room temperature for 30 minutes
  9. customAfter completion of the reaction
  10. washthe resin was thoroughly washed with methylene chloride, dimethylformamide (DMF) and 20% aqueous ethanol

출처 및 근거

ORD 기록
ord-667291f776064bb6b6d0d90a4de81add
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07645614B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트